CN103773957B - Precipitating alum and removing iron technique in Zinc hydrometallurgy process - Google Patents
Precipitating alum and removing iron technique in Zinc hydrometallurgy process Download PDFInfo
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- CN103773957B CN103773957B CN201410040629.9A CN201410040629A CN103773957B CN 103773957 B CN103773957 B CN 103773957B CN 201410040629 A CN201410040629 A CN 201410040629A CN 103773957 B CN103773957 B CN 103773957B
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Abstract
Precipitating alum and removing iron technique in a kind of Zinc hydrometallurgy process of the present invention, comprises the following steps: regulate heavy alum supernatant liquor pH value, add oxidant reaction, regulate reaction solution PH=4.8 ~ 5.2, precipitate deironing, regulate heavy alum supernatant liquor PH=3.5 ~ 4.5; Described oxygenant is H
2o
2oxygenant or H
2o
2with the agent of manganese powder co-oxidation, temperature of reaction is 60 ~ 70 DEG C, stirring reaction 40 ~ 90min.Use H
2o
2oxygenant or H
2o
2with manganese powder co-oxidation agent Oxidation of Fe
2+for Fe
3+formation siderotil is removed, and cost is low, can mn ion content in reduction system, mn ion in system is effectively controlled 5 ~ 6g/l in processing requirement, effective minimizing systemic circulation amount, reduce zinc content in acid leaching residue, iron vitriol slag, both improved zinc metal recovery rate, improve Faradaic current efficiency again, reduce power consumption, operation is simplified.
Description
Technical field
The invention belongs to smelting field of nonferrous metal, be specifically related to the utilization of precipitating alum and removing iron process oxidant in Zinc hydrometallurgy process.
Background technology
Zinc hydrometallurgy smelts the main method in zinc, and current have 80% of zinc output all to come from Zinc hydrometallurgy process, and zinc hydrometallurgy generally comprises the steps such as leaching, pre-neutralization, precipitating alum and removing iron, and its technique is substantially identical, and the key distinction is to adopt diverse ways deironing.Meutral innersion after zinc ore roasting, in leach liquor, iron content is few, but the leaching yield of zinc is also very low.Current technique generally uses zinc baking sand hot acid to leach, and the leaching yield of zinc improves greatly, but a large amount of iron also thereupon leach enter solution.Manganese powder is added, by Fe in acid leaching solution
2+be oxidized to Fe
3+, Fe under solutions of weak acidity
3+siderotil can be formed be removed.
In zinc ore, frequent sulfur-bearing and ferrous iron are measured high, cause needing to add more manganese powder in acid leaching solution, mn ion content straight line in solution is made to increase, record content maximum during production and reach 24g/l, for removing mn ion makes electrolysis power mono-consumption reach 3400Kwh/t.Zn, cause energy waste.
Summary of the invention
The present invention be directed to deficiency of the prior art, provide that a kind of cost is low, power consumption less, the method for deironing in the simple Zinc hydrometallurgy process of operation.
The present invention is achieved by the following technical solutions:
Precipitating alum and removing iron technique in Zinc hydrometallurgy process, comprises the following steps: regulate heavy alum supernatant liquor PH=3.5 ~ 4.5, add Fe
2+oxygenant react, temperature of reaction is 60 ~ 70 DEG C, stirring reaction 40 ~ 90min, regulate reaction solution PH=4.8 ~ 5.2, precipitation deironing, it is characterized in that: described Fe
2+oxygenant be H
2o
2oxygenant or H
2o
2with the agent of manganese powder co-oxidation.
More specifically, described oxygenant is H
2o
2oxygenant, feed postition for add H bottom described heavy alum supernatant liquor
2o
2solution, H
2o
2add-on be Oxidation of Fe
2+1.3 ~ 2.1 times of theoretical amount.
Described oxygenant is H
2o
2with the agent of manganese powder co-oxidation, feed postition is for first to add Oxidation of Fe
2+the manganese powder of theoretical amount 30%-60%, then adds H bottom described heavy alum supernatant liquor
2o
2solution, H
2o
2amount be Oxidation of Fe
2+1.1 ~ 2.0 times of theoretical amount.
Wherein a kind of add-on is, the add-on of described manganese powder is Oxidation of Fe
2+30% of theoretical amount, described H
2o
2add-on be Oxidation of Fe
2+1.8 ~ 2.0 times of theoretical amount.
In another, add-on is: the add-on of described manganese powder is Oxidation of Fe
2+60% of theoretical amount, described H
2o
2add-on be Oxidation of Fe
2+1.1 ~ 1.3 times of theoretical amount.
More specifically, heavy alum supernatant liquor PH=4 is regulated.
Test is utilized to set forth technique scheme below:
Test equipment used:
Thermostatic type electric heater one; Mercurythermometer one; 5L wide mouth beaker two; One, controllable type agitator.
One, H
2o
2the impact of solution feed postition
Process of the test:
(1) a certain amount of heavy alum supernatant liquor is got.
(2) assay sinks Fe in alum supernatant liquor
2+content.
(3) according to Fe in heavy alum supernatant liquor
2+cubage add H
2o
2amount.
(4) massfraction added in heavy alum supernatant liquor is the H of 27.5%
2o
2solution, feed postition is for add from heavy alum supernatant liquor surface.
(5) heavy alum supernatant liquor temperature is controlled 60 ~ 70 DEG C, pH value controls 2.0 ~ 2.5.
(6) when reacted between when reaching 40 minutes, Fe in the heavy alum supernatant liquor of chemical examination
2+content.
Concrete data are in table 1:
Conclusion: in PH=2.0 ~ 2.5, feed postition is that heavy alum supernatant liquor surface adds, temperature 60 ~ 70 DEG C, H
2o
2consumption is 8 times of theoretical addition amount, Fe after deironing
2+content is all not less than 30mg/l, and de-ferrous effect is bad.
By H
2o
2amount ranges test when being set as 1.0 ~ 2.5 times of theoretical amount.Meanwhile, feed postition is made into the bottom that addition point is solution, reaction conditions is: heavy alum supernatant liquor is containing Fe
2+: 1g/l, temperature: 70 DEG C, reaction times: 40min, solution PH=3.5.The results are shown in Table 2
Test proves H
2o
2oxygenant adds to bottom heavy alum supernatant liquor better than liquid level.This is because H
2o
2the proportion of solution is less than heavy alum supernatant liquor proportion, is added on liquid level, with the Fe in solution
2+contacted with ions is bad, easily decomposes; Be added on bottom heavy alum supernatant liquor, thereon in floating process, same to Fe
2+reaction, add stirring action, oxidation effectiveness is better.Meanwhile, when determining that this type material consumption reaches 1.6 times of theoretical amount by test, iron-removal rate, to 99.86%, after this increases H
2o
2the consumption of oxygenant, deironing rate raises not obvious.
Two, the impact of pH value
(1) reaction conditions is for heavy alum supernatant liquor is containing Fe
2+: 1g/l, temperature: 70 DEG C, reaction times: 40min, H
2o
2oxygenant consumption is certain, and initial pH is tested in 1 ~ 5 scope, the results are shown in Table 3
2) impact of terminal pH value
Terminal pH value is higher, and deironing rate is higher.But terminal pH value can not be too high, otherwise zinc can be hydrolyzed, and terminal pH value should control 4.8 ~ 5.2.
Three, the impact of temperature
Reaction conditions is Fe in heavy alum supernatant liquor
2+: 1g/l, reaction times: 40min, pH value: 4.0 ~ 4.5, temperature: the scope of 40 ~ 90 DEG C is tested, and acquired results is in table 4.
Conclusion: deironing rate is higher when temperature is 60 ~ 70 DEG C, can meet middle leaching operation need of production.Temperature is too low, and speed of response is slow, and de-ferrous effect is poor.Temperature is higher than after 70 DEG C, and along with temperature raises, deironing rate reduces.This is due to H
2o
2oxygenant decomposes Cheng Shui and oxygen, temperature is higher, and decomposition rate is faster, and therefore oxidation capacity declines, and de-ferrous effect is deteriorated.
Four, H
2o
2with manganese powder co-oxidation agent deironing
Test conditions is: solution pH value: 3.5 ~ 4.0, temperature of reaction: 60 ~ 70 DEG C, H
2o
2liquid quality fraction is 27.5%, and it the results are shown in Table 5:
Conclusion: manganese powder add-on is 0.6 times of theoretical addition amount, H
2o
2when oxygenant is 1.6 times of theoretical addition amount, the Fe in heavy alum supernatant liquor
2+can effective oxidized removing.
The beneficial effect that in Zinc hydrometallurgy process of the present invention, precipitating alum and removing iron novel process obtains has:
(1) can mn ion content in reduction system, mn ion content can be controlled within 5 ~ 6g/l, improve Faradaic current efficiency, reduce power consumption.
(2) H
2o
2oxidant cost is lower, do not produce additional impurities, and operational safety is reliable, site environment is clean, energy-conserving and environment-protective.
(3) avoid other substance reaction in excessive manganese powder and heavy alum supernatant liquor, cause the complicated of operation.
Embodiment
Embodiment one
Fe in heavy alum supernatant liquor
2+content is 0.6 ~ 1.34g/l, and regulate PH=4.0, temperature: 70 DEG C, adds the H equaling theoretical amount 1.6 times bottom heavy alum supernatant liquor
2o
2solution, reaction times 40min, deironing rate is in table 6:
Embodiment two
Manganese powder add-on is 60%, H of theoretical addition amount
2o
2h when oxygenant add-on is 1.1 ~ 1.3 times of theoretical addition amount
2o
2oxygenant commerical test data, reaction conditions is heavy alum supernatant liquor pH value: 4.0, temperature: 70 DEG C, H
2o
2solution is industrial hydrogen peroxide.The results are shown in Table 7:
Embodiment three
Manganese powder add-on be theory add 30%, H
2o
2oxygenant add-on is 1.8 ~ 2.0 times of theoretical addition amount, and reaction conditions is heavy alum supernatant liquor pH value: 4.0, temperature: 70 DEG C, H
2o
2solution is industrial hydrogen peroxide.The results are shown in Table 8:
As can be seen from table 7 and table 8, when oxidation trough manganese powder add-on is 60% of theoretical addition amount, H
2o
2when oxygenant add-on is 1.0 ~ 1.3 times of theoretical addition amount, by oxidation solution flow 220m
3/ h, heavy alum supernatant Fe
2+1g/l, cathode zinc 340t/d calculate, H
2o
2oxygenant unit consumption is 19.18 ㎏/t.Zn, and co-oxidation agent is to Fe
2+oxidation ratio be 92%; When oxidation trough manganese powder add-on is 30%, H of theoretical addition amount
2o
2when oxygenant add-on is 1.8 ~ 2.0 times of theoretical addition amount, H
2o
2oxygenant unit consumption amount is 29.51 ㎏/t.Zn, and co-oxidation agent is to Fe
2+oxidation ratio be 89%.
Can cost be carried out by above-described embodiment data and economic benefit calculation as follows:
1, cost
(1) manganese powder iron removal by oxidation cost, is used
Fe in heavy alum supernatant liquor
2+calculate by 1g/l, cathode zinc output is pressed 340t/d and is calculated, and manganese powder unit consumption is 39.03 ㎏/t.Zn, and unit cost is 62.57 yuan/t.Zn.
(2), manganese powder and H
2o
2conbined usage deironing cost
When manganese powder add-on is theoretical addition amount 60%, Fe in heavy alum supernatant liquor
2+calculate by 1g/l, cathode zinc output press 340t/d calculating, and manganese powder unit consumption is 15.56 ㎏/t.Zn, and unit cost is 24.94 yuan/t.Zn, H
2o
2when oxygenant add-on is 1.0 ~ 1.3 times of theoretical addition amount, H
2o
2oxygenant unit consumption is 19.18 ㎏/t.Zn, H
2o
2oxygenant unit cost is 28.77 yuan/t, and total cost is 53.71 yuan/t.Zn.
2, economic benefit
(1), direct benefit
Calculate can produce economic benefit by annual output 100000 tons of cathode zinc:
(62.57-53.71) × 100000=88.6(ten thousand yuan)
(2), indirect benefit
Can mn ion content in reduction system, mn ion in system is effectively controlled 5 ~ 6g/l in processing requirement, effectively reduces systemic circulation amount, reduce two slags (acid leaching residue, iron vitriol slag) containing zinc, both improve zinc metal recovery rate, improved Faradaic current efficiency again, reduce power consumption.
Can learn, use H
2o
2with manganese powder associating proportioning, additive use cost can be reduced, can production capacity be increased again, reduce unit dc consumption, best de-ferrous effect can be played again.
Claims (4)
1. a precipitating alum and removing iron technique in Zinc hydrometallurgy process, comprises the following steps: regulate heavy alum supernatant liquor pH=3.5 ~ 4.5, add Fe
2+oxygenant react, temperature of reaction is 60 ~ 70 DEG C, stirring reaction 40 ~ 90min, regulate reaction solution pH=4.8 ~ 5.2, precipitation deironing, it is characterized in that: described Fe
2+oxygenant be H
2o
2with the agent of manganese powder co-oxidation, feed postition is for first to add Oxidation of Fe
2+the manganese powder of theoretical amount 30% ~ 60%, then adds H bottom described heavy alum supernatant liquor
2o
2solution, described H
2o
2add-on be Oxidation of Fe
2+1.1 ~ 2.0 times of theoretical amount.
2. precipitating alum and removing iron technique in Zinc hydrometallurgy process according to claim 1, is characterized in that: the add-on of described manganese powder is Oxidation of Fe
2+30% of theoretical amount, described H
2o
2add-on be Oxidation of Fe
2+1.8 ~ 2.0 times of theoretical amount.
3. precipitating alum and removing iron technique in Zinc hydrometallurgy process according to claim 1, is characterized in that: the add-on of described manganese powder is Oxidation of Fe
2+60% of theoretical amount, described H
2o
2add-on be Oxidation of Fe
2+1.1 ~ 1.3 times of theoretical amount.
4. precipitating alum and removing iron technique in Zinc hydrometallurgy process according to claim 1, is characterized in that: regulate heavy alum supernatant liquor pH=4.
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| CN107177734A (en) * | 2017-06-07 | 2017-09-19 | 云南金鼎锌业有限公司 | A kind of method and apparatus that iron is removed in zinc abstraction technique |
| CN112176184A (en) * | 2020-09-09 | 2021-01-05 | 安阳岷山环能高科有限公司 | Method for removing iron by combining oxygen and hydrogen peroxide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101413059A (en) * | 2008-11-27 | 2009-04-22 | 郴州丰越有色金属冶炼有限公司 | Process for comprehensively and efficiently recycling zinc and indium in indium raffinate |
| CN101709382A (en) * | 2009-12-17 | 2010-05-19 | 新乡超能电源有限公司 | Recovery and comprehensive treatment process of valuable metals in zinciferous materials |
| CN101838736A (en) * | 2010-06-01 | 2010-09-22 | 河南豫光锌业有限公司 | Wet separation method for valuable metals in purified liquid cobalt slags of wet zinc smelting system |
| CN103468951A (en) * | 2013-08-21 | 2013-12-25 | 黄石大江集团有限公司 | Pseudo goethite method for removing iron in zinc leaching solution |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101413059A (en) * | 2008-11-27 | 2009-04-22 | 郴州丰越有色金属冶炼有限公司 | Process for comprehensively and efficiently recycling zinc and indium in indium raffinate |
| CN101709382A (en) * | 2009-12-17 | 2010-05-19 | 新乡超能电源有限公司 | Recovery and comprehensive treatment process of valuable metals in zinciferous materials |
| CN101838736A (en) * | 2010-06-01 | 2010-09-22 | 河南豫光锌业有限公司 | Wet separation method for valuable metals in purified liquid cobalt slags of wet zinc smelting system |
| CN103468951A (en) * | 2013-08-21 | 2013-12-25 | 黄石大江集团有限公司 | Pseudo goethite method for removing iron in zinc leaching solution |
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